EP2017659B1 - A fibre optic sensor and method for making - Google Patents

A fibre optic sensor and method for making Download PDF

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Publication number
EP2017659B1
EP2017659B1 EP08156110.2A EP08156110A EP2017659B1 EP 2017659 B1 EP2017659 B1 EP 2017659B1 EP 08156110 A EP08156110 A EP 08156110A EP 2017659 B1 EP2017659 B1 EP 2017659B1
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EP
European Patent Office
Prior art keywords
ceramic material
fiber
optical
optical agents
open pore
Prior art date
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Ceased
Application number
EP08156110.2A
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German (de)
English (en)
French (fr)
Other versions
EP2017659A1 (en
Inventor
James Scott Vartuli
Kenneth Sherwood Bousman
Kung-Li Deng
Kevin Paul Mcevoy
Hua Xia
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General Electric Co
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General Electric Co
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/7703—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator using reagent-clad optical fibres or optical waveguides
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10—Coating
    • C03C25/104—Coating to obtain optical fibres
    • C03C25/106—Single coatings
    • C03C25/1061—Inorganic coatings
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10—Coating
    • C03C25/12—General methods of coating; Devices therefor
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
    • G02B6/02—Optical fibres with cladding with or without a coating
    • G02B6/02057—Optical fibres with cladding with or without a coating comprising gratings
    • G02B6/02076—Refractive index modulation gratings, e.g. Bragg gratings
    • G02B6/0208—Refractive index modulation gratings, e.g. Bragg gratings characterised by their structure, wavelength response
    • G02B6/021—Refractive index modulation gratings, e.g. Bragg gratings characterised by their structure, wavelength response characterised by the core or cladding or coating, e.g. materials, radial refractive index profiles, cladding shape
    • G02B6/02104—Refractive index modulation gratings, e.g. Bragg gratings characterised by their structure, wavelength response characterised by the core or cladding or coating, e.g. materials, radial refractive index profiles, cladding shape characterised by the coating external to the cladding, e.g. coating influences grating properties
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/7703—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator using reagent-clad optical fibres or optical waveguides
    • G01N2021/7706—Reagent provision
    • G01N2021/7726—Porous glass

Definitions

  • This invention relates generally to a method for making a fiber optic sensor and more particularly, for a fiber optic sensor for harsh environments.
  • Fiber optic sensors may be used to monitor dynamic chemical and physical processes that are associated with changes in an environment.
  • a typical fiber optic sensor positions a sensor material, with the assistance of one or more types of support, to interact with the substance or environment that is being monitored, measured and/or detected.
  • a chemical fiber optic sensor contains an optical agent that identifies optical index changes based upon unique chemical environments. To function properly, the optical agent must be in an optically clear support structure that holds the optical agent and permits the optical agent to interact with the environment or substance being monitored, measured or detected.
  • U.S. Patent No. 5,496,997 to Pope discloses an optical fiber where the distal end of the fiber is coupled to amorphous silica microspheres by an adhesive material.
  • the sensor can fail in harsh environments, as the adhesive layer may break down at high temperatures or in the harsh environments.
  • fiber optic sensor comprising a fiber having a cladding and a modified surface integral with the fiber, wherein the fiber surface is modified by applying ceramic material, said modified surface comprising an open pore network and optical agents dispersed within the open pores of the open pore network, wherein the modified surface is intimately bonded to the fibre surface and wherein the optical agents comprise a Group 8-10 transition metal or a metal oxide selected from the group consisting of tin dioxide, yttrium oxide, vanadium oxide, titanium oxide and tungsten oxide and said modified surface is on the cladding.
  • a process for making a fiber optic sensor comprising applying ceramic material to a fiber having a cladding and forming an open pore network structure, dispersing optical agents within the pores of the open pore network and integrating the ceramic material with the fiber, wherein the step of applying ceramic material consists of applying ceramic material or a mixture comprising ceramic material and optical agents to the cladding such that the modified surface is intimately bonded to the fibre surface; and wherein said optical agents comprise a Group 8-10 transition metal or a metal oxide selected from the group consisting of tin dioxide, yttrium oxide, vanadium oxide, titanium oxide and tungsten oxide.
  • the various embodiments provide fiber optic sensors that can withstand high temperatures and harsh environments.
  • a fiber optic sensor comprises a fiber having a modified surface integral with the fiber, said modified surface comprising an open pore network and optical agents disposed within the open pores of the open pore network.
  • a fiber optic sensor may be used to measure physical, electrical and chemical parameters.
  • the fiber optic sensor is a chemical fiber optic sensor.
  • a fiber comprises a fiber core and a fiber cladding.
  • the fiber cladding at least partly surrounds the fiber core, which forms a waveguide that extends longitudinally along an axis and includes parts having variations in refractive index (or optical thickness) to form an optical diffraction grating.
  • the fiber core is transparent and may comprise sapphire, a porous sol-gel glass or a fused silica material.
  • the fiber cladding may be transparent and may be made of the same material as the core, but with a low refractive index.
  • the fiber cladding comprises glass or silica.
  • the modified surface is on the fiber cladding of the fiber.
  • the modification to the fiber comprises applying a ceramic material to the surface of the fiber in any conventional manner. As the ceramic material solidifies, it forms a porous and optically clear support structure, which is a three-dimensional matrix or lattice type structure with a plurality of interconnecting pores that extend completely throughout the support structure and create an open pore network.
  • the pore sizes may be any size suitable for allowing a sensing gas to pass through the support structure.
  • the pore sizes are up to about 150 nm in diameter.
  • the pores sizes are from about 1 nm to about 150 nm in diameter.
  • the pore sizes may be controlled in a conventional manner by adjusting the time and temperature while the material is solidifying.
  • the ceramic material is applied by spraying, brushing, rolling, pouring, dipping, immersing coating or applying a film to a surface of the fiber.
  • a surface of the fiber is modified by coating the surface.
  • a surface is modified by dipping the fiber.
  • a surface is modified by forming a film on the surface.
  • the ceramic material may be silica, alumina or titania.
  • the alumina, titania and silica may be derived from an organo-metallic, such as a tetraethoxyorthosilicate.
  • the ceramic material comprises silica.
  • Optical agents are sensors that chemically sense unique chemical environments and measure the optical index of the fiber cladding.
  • Optical agents may be any type of sensor that is known in the art.
  • the optical agents may be metals or transition metals.
  • the transition metal is any compound comprising Group 8-10 transition metals, such as ruthenium, rhodium, platinum and palladium.
  • the optical agent is palladium.
  • the optical agent may include a metal oxide.
  • the metal oxide may include tin dioxide, yittrium oxide, vanadium oxide, titanium oxide and tungsten oxide.
  • the optical agents are disposed within the open pores of the open pore network and are at least partially exposed to the ambient air.
  • Optical agents are disposed into the open pores by dispersing the optical agents into the open pore network by any conventional method.
  • the optical agents may be dispersed by spraying, brushing, rolling, pouring, dipping, immersing or coating the modified surface with the optical agents.
  • the optical agents are dispersed within the pores of the open pore network by dipping the modified fiber optic into a solution comprising optical agents.
  • the solution may be prepared by blending optical agents with water or alcohol.
  • the ceramic material is integrated with the fiber by intimately bonding the ceramic material to a fiber surface without the need for adhesive materials or adhesive layers.
  • the ceramic material infiltrates the surface of the fiber to form an integrated and modified surface on the fiber that effectively replaces the fiber surface with the new modified surface.
  • the ceramic material may be integrated with the fiber by any means suitable for densifying and intimately bonding the ceramic material to a fiber surface.
  • the densified ceramic material forms an open pore network within a dense structure that holds the optical agents in place and provides access to the environment or substance that is to be measured, monitored or detected. This open pore network holds and protects the optical agents in a support structure that is thermally, chemically and mechanically robust and stable.
  • the ceramic material may be densified and bonded to the fiber by heat treatment, drying or irradiation. In another embodiment, the ceramic material is heat treated. Heat treatment may be made in any conventional manner. In one embodiment, the modified fiber is heated between about 300°C and about 600°C for up to about 4 hours. In one embodiment, the modified fiber is heated for about 1 to about 3 hours. Continued heating at higher temperatures or for longer times will eventually cause the open pore network to become fully dense having little or no porosity.
  • a process for making a fiber optic sensor comprises applying ceramic material to a fiber to form an open pore network structure, dispersing optical agents within the pores of the open pore network and integrating the ceramic material with the fiber.
  • the ceramic material may be silica, alumina or titania.
  • the alumina, titania and silica may be derived from an organo-metallic, such as a tetraethoxyorthosilicate.
  • the ceramic material comprises spherical particles having diameters in a range from about 20 nm to about 700 nm. The diameters are measured by a scanning electron microscope. In one embodiment, the spherical particles are monosized. In another embodiment, at least about 95% of the spherical particles are within about 10% of the mean diameter of the spherical particles.
  • the ceramic material comprises spherical particles of silica.
  • Spherical particles of silica may be made by adding a silica precursor, such as tetraethoxyorthosilicate, into a solution comprising alcohol and optionally, water from about 1 to about 50 percent by weight ammonia. The size of the particles is controlled by the relative concentrations of water, ammonia and alcohol.
  • the alcohol is ethanol.
  • the amount of alcohol is in the range of from about 10 to about 70 percent by weight based on the weight of the solution.
  • the amount of ammonia is present from about 1 to about 50 percent by weight based on the weight of the solution.
  • the amount of water is present from about 10 to about 70 percent by weight based on the weight of the solution.
  • the amount of silica precursor is present from about 1 to about 10 percent by weight based on the weight of the solution.
  • the ceramic material comprising spherical particles is applied by spraying, brushing, rolling, pouring, dipping, immersing coating or applying a film to a surface of the fiber.
  • a surface of the fiber is modified by dipping the fiber into an aqueous solution of ceramic spherical particles. The spherical particles adhere to the surface of the fiber through van der Waals forces. As the water from the solution dries, capillary forces from the evaporating water film pull the spherical particles into a dense network of touching particles and open spaces forming open pores.
  • the optical agents are dispersed within the open pores of the open pore network by any conventional method. As stated above, the optical agents may be dispersed by spraying, brushing, rolling, pouring, dipping, immersing or coating the modified surface with the optical agents. In one embodiment, the optical agent is dispersed within the open pore network by solution. The optical agents are added to a solution comprising water or alcohol and the fiber with the modified surface is dipped into the solution. Repeated steps of dispersing the optical agent into the open pore network may be used to increase the concentration of the optical agents on the fiber. The optical agents are situated within the open pores of the open pore network and are at least partially exposed to the environment or substance to be measured.
  • the ceramic material is integrated with a fiber surface by any means suitable for densifying and intimately bonding the ceramic material to the fiber without the need for adhesive materials or adhesive layers.
  • Figure 1A is a diagram depicting a fiber 10 before heat treatment.
  • the surface of the fiber 10 is modified by the application of a ceramic material 20 comprising ceramic spherical particles.
  • the ceramic particles 20 adhere to the surface of the fiber 10 and form an open pore network of touching particles and open spaces 30.
  • Optical agents 40 are dispersed within the open pores 30 of the open pore network.
  • Figure 1B is a diagram depicting the fiber optic 10 after heat treatment.
  • the ceramic spherical particles 20 densify and integrate with the fiber 10 to form an open pore network within a dense ceramic material 20.
  • the optical agents 40 are supported and held in place by the open pore network in the ceramic material 20 and are exposed to the environment or substance to be measured.
  • a process for making a fiber optic sensor comprises applying a ceramic material mixture comprising ceramic material and optical agents to a fiber, forming an open pore network structure within the ceramic material and integrating the ceramic material with the fiber.
  • the ceramic material mixture comprises ceramic material and optical agents.
  • the ceramic material mixture is prepared by adding optical agents to the ceramic material.
  • the optical agents may be blended with the ceramic material in any conventional manner.
  • the optical agents and ceramic material are blended together in solution.
  • a solution of tetraethoxyorthosilicate, alcohol and optical agents is prepared.
  • the ceramic material mixture is applied to a fiber surface in any conventional manner.
  • the ceramic material is applied by spraying, brushing, rolling, pouring, dipping, immersing coating or applying a film to the surface.
  • the ceramic material mixture is applied by coating the surface of the fiber.
  • the ceramic material mixture is applied by dipping the fiber.
  • a film comprising the ceramic material mixture is formed on the surface of the fiber.
  • the open pore network may be formed by any suitable means for hardening ceramic material, such as drying or heat treating. As the ceramic material dries or is heated, the ceramic material begins to gel and cracks begin to form in the ceramic material. The cracks provide an open pore network within the dense ceramic material. The amount of cracking can be controlled by the rate of change of humidity and by the heat or drying rate.
  • the ceramic material is integrated with the fiber optic by any means suitable for densifying and intimately bonding the ceramic material to the fiber without the need for adhesive materials or adhesive layers.
  • the ceramic material mixture further comprises a polymer.
  • the polymer may be any type of organic polymer that will decompose at elevated temperatures, such as during a heat treatment step.
  • the organic polymer may be oxides of polyolefins, latex polymers, polyesters and polypropylenes.
  • the organic polymer includes polyethylene oxide or polypropylene oxide. The polymer may be added to the ceramic material in an amount of from about 0.1 to about 10 percent by volume based on the ceramic material.
  • the polymer aids in producing an open pore network within a dense ceramic material by causing cracks and voids to form in the ceramic coating.
  • the ceramic material is heat treated in any conventional manner and the polymer will decompose during the heat treating step and leave voids in the coating, which will increase the open pores within the dense ceramic coating.
  • the voids and cracks within the ceramic coating are large enough to allow gas to diffuse through the voids, but are small enough to not cause structural damage to the ceramic coating.
  • the voids may be from about 10 ⁇ in diameter to about 100 ⁇ in diameter.
  • Figure 2A is a diagram depicting a fiber 200 before heat treatment.
  • a mixture of a ceramic material 210, optical agents 220 and a polymer 230 are applied to the surface of a fiber 200 and allowed to dry under a controlled humidity to induce cracking (not shown) in the dense ceramic material.
  • Figure 2B is a diagram depicting a fiber 200 after heat treatment.
  • the modified surface is heat treated and during heat treatment, the ceramic material 210 densifies and intimately bonds with the fiber optic 200.
  • the polymer 230 decomposes leaving voids 240 in the ceramic material 210.
  • the optical agents 220 are supported and held in place within the open pore network formed within the ceramic material 210 and are exposed to the environment or substance to be measured.
  • a mixture of 89.5 percent by weight tetraethoxyorthosilicate, 10.5 percent by weight palladium and 40 percent by weight based on the weight of the tetraethoxyorthosilicate and palladium of 1-propanol was prepared.
  • a film of the mixture of silica and palladium was applied to a glass substrate and heat treated at 400°C for 2 hours.
  • the film thickness was about 100 ⁇ m.
  • Figures 3-8 show the H 2 response optical reflection curve between alternating 5% H 2 in N 2 gas at 25°C (room temperature), 120°C, 172°C, 355°C, 425°C and 525°C, respectively.
  • the sensor measured H 2 sensing up to about 355°C.
  • the relative response to the H 2 gas is summarized in Figure 9 .
  • the relative response which is the quotient of the change of signal to the signal level.
  • the values are evaluated by the average using the faster change signal. The results show that in the temperature range where the film is capable of sensing, sensitivity increases with increasing temperatures.
  • Figure 10 is the response time over temperature.
  • the response time values are evaluated by an average using the faster change signal. The results show that within the temperature where the film is capable of sensing, the higher the temperature, the shorter the response time, which corresponds to the increasing chemical reaction rate at the elevated temperature.
  • Prior art Pd-alloy based sensing materials interact with hydrogen at room temperature allowing the detection and measurement of hydrogen by optical and fiberoptic techniques, but do not show detection at higher temperatures.
  • a mixture of 80 percent by weight tetraethoxyorthosilicate, 15 percent by weight tin dioxide, 5 percent by weight palladium and 8 percent by weight based on the weight of the tetraethoxyorthosilicate, palladium and tin dioxide of 1-propanol was prepared.
  • a film of the mixture of silica, tin dioxide and palladium was applied to a glass substrate and heat treated at 400°C for 2 hours.
  • the film thickness was about 20 ⁇ m.
  • the fiber optic sensor was tested for carbon monoxide responses between 325°C and 525°C.
  • Figures 11 and 12 show the CO response optical reflection curve between alternating 5% CO in N 2 gas at 425°C and 525°C, respectively.
  • the sensor measured CO sensing across the temperature range.
  • a mixture of 89.5 percent by weight tetraethoxyorthosilicate, 10.5 percent by weight palladium and 20 percent by weight based on the weight of the tetraethoxyorthosilicate and palladium of 1-propanol was prepared.
  • a film of the mixture of silica and palladium was applied to a glass substrate and heat treated at 500 °C for 2 hours.
  • the film thickness was about 100 ⁇ m.
  • FIG. 13 and 14 show the CO response optical absorption curve between alternating 5% CO in N 2 gas at 280°C and 525°C, respectively. As shown in Figure 14 , the response to the CO gas is quick and big.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • General Physics & Mathematics (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Optics & Photonics (AREA)
  • Inorganic Chemistry (AREA)
  • Plasma & Fusion (AREA)
  • Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
  • Optical Fibers, Optical Fiber Cores, And Optical Fiber Bundles (AREA)
EP08156110.2A 2007-07-20 2008-05-13 A fibre optic sensor and method for making Ceased EP2017659B1 (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US11/780,701 US7720321B2 (en) 2007-07-20 2007-07-20 Fiber optic sensor and method for making

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EP2017659A1 EP2017659A1 (en) 2009-01-21
EP2017659B1 true EP2017659B1 (en) 2016-03-30

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EP (1) EP2017659B1 (enExample)
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JP6915859B2 (ja) * 2017-08-08 2021-08-04 学校法人 創価大学 光ファイバ水素センサ及びその製造方法
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US20090022449A1 (en) 2009-01-22
JP2009025289A (ja) 2009-02-05
CN101349649B (zh) 2013-05-29
JP5025561B2 (ja) 2012-09-12
CN101349649A (zh) 2009-01-21
US7720321B2 (en) 2010-05-18
EP2017659A1 (en) 2009-01-21

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